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ChemicalBook CAS DataBase List FMOC-DOPA(ACETONIDE)-OH

FMOC-DOPA(ACETONIDE)-OH synthesis

4synthesis methods
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Yield:852288-18-7 90 %Chromat.

Reaction Conditions:

in toluene at 80; under 225.023 Torr; for 0.416667 h;Inert atmosphere;Sealed tube;Molecular sieve;Temperature;Reagent/catalyst;Solvent;Pressure;

Steps:

1.2; 2.2; 3.2
(2) taking the above dried Fmoc-DOPA-OH (2.1 g, 5 mmol) intermediate,a magnetic stirrer, and DMP (6.13ml, 50mmol),Add to a 100ml two-necked flask,Add a rectifying head to the vertical bottle opening of the flask.The outlet of the distillation head is connected to an oil seal.The side bottle mouth is sealed with a rubber stopper for sampling. After argon gas is applied for 5 minutes, 50 ml of anhydrous toluene (3A molecular sieve drying) is added to make a methanol tape.Continue to argon for 20 minutes. Then, depressurize to about 300hPa,The oil bath was heated to an oil temperature of 80 ° C, and no additional catalyst was added.The progress of the reaction was monitored by thin layer chromatography (TLC).And compared with Fmoc-DOPA (Acetonide)-OH standard.When the temperature rises to 115 ° C, the liquid begins to distill,After 15 minutes, 10-13 ml of liquid was distilled off.After 1 hour of reaction, the yield by TLC was about 90%.

References:

Hainan University;Liu Zhongqiang;He Yanmiao;Hu Bihuang;Chen Sikang;Zhong Shibo;Wan Ying;Yao Rui;Li Mengdi CN110041300, 2019, A Location in patent:Paragraph 0066; 0068-0069; 0071-0072; 0074

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